CN108609594B - Method for treating and recycling wastewater in iron phosphate production - Google Patents
Method for treating and recycling wastewater in iron phosphate production Download PDFInfo
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- CN108609594B CN108609594B CN201810268328.XA CN201810268328A CN108609594B CN 108609594 B CN108609594 B CN 108609594B CN 201810268328 A CN201810268328 A CN 201810268328A CN 108609594 B CN108609594 B CN 108609594B
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- iron phosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
Abstract
A method for treating and recycling wastewater in iron phosphate production comprises the following steps: feeding washing water containing hydrochloric acid in the iron phosphate production into an electrolytic cell to obtain chlorine; introducing chlorine into the yellow phosphorus water, and absorbing the chlorine by the yellow phosphorus water to obtain a mixture of phosphoric acid and hydrochloric acid; reacting a mixture of phosphoric acid and hydrochloric acid with the sulfuric acid cinder to obtain crude iron phosphate; according to the invention, after hydrochloric acid, phosphorus chloride, magnesium chloride and calcium chloride in the primary washing water are subjected to electrolytic reaction, chloride ions generate chlorine, the chlorine reacts with yellow phosphorus water to generate a mixture of first phosphoric acid and third hydrochloric acid, and the mixture of the first phosphoric acid and the third hydrochloric acid and sulfuric acid cinder generate crude iron phosphate, so that the sulfuric acid cinder is changed into valuable through recycling of the chloride ions, the discharge of the chloride ions is avoided to pollute the environment, cations are combined with hydroxyl to form precipitates to be discharged, the concentration of the cations is prevented from being increased continuously, the primary washing water subjected to electrolytic treatment can be recycled, and the zero emission of the washing water is realized.
Description
Technical Field
The invention relates to the technical field of iron phosphate preparation, in particular to a method for treating and recycling wastewater in iron phosphate production.
Background
The iron phosphate can be used as an iron source for preparing the lithium iron phosphate serving as the cathode material of the lithium ion battery, but the cost is high, only the iron phosphate occupies about half of the cost of the raw materials, the cost of the iron phosphate must be greatly reduced, and the market demand is met with high cost performance. The sulfuric acid cinder is the residue discharged after roasting pyrite to extract sulfur. Iron is the main available component in the clinker. At present, the comprehensive utilization of the sulfuric acid cinder is not ideal, and most of the sulfuric acid cinder is subjected to landfill treatment except for a small part of the sulfuric acid cinder used as iron making and building materials, so that the waste of resources and the environmental pollution are caused. The sulfuric acid cinder is used as a raw material for preparing the iron phosphate, and no report is found. The iron phosphate is required to be washed in the production process, the washing water contains low-concentration hydrochloric acid and chloride salt, if the washing water is not treated, the washing water cannot be recycled, and the hydrochloric acid and the chloride salt have low concentration, the washing water is difficult to treat by a conventional method, such as a neutralization replacement method, that is, a large amount of lime is adopted to perform a neutralization reaction with waste hydrochloric acid. The method for treating the hydrochloric acid in the wastewater has high treatment cost and low recovery value, can generate a large amount of wastewater to pollute the environment, can cause resource waste and certain influence on the environment by direct discharge, and particularly has prominent pollution of chloride ions to the environment.
Disclosure of Invention
In view of the above, there is a need to provide a method for wastewater treatment and recycling in iron phosphate production, which can prepare iron phosphate from sulfuric acid cinder, effectively recycle hydrochloric acid and washing water in iron phosphate washing water, and meet zero emission of pollutants, especially zero emission of chloride ions.
A method for treating and recycling wastewater in iron phosphate production comprises the following steps:
the method comprises the following steps: feeding the primary washing water into an electrolysis device for electrolysis to obtain chlorine, hydrogen, hydroxide precipitates and secondary washing water, discharging the hydrogen from a hydrogen discharge port, and discharging the hydroxide precipitates from an electrolysis bath;
the method comprises the following steps of (1) preparing primary washing water, wherein the primary washing water is washing water containing 1-5% of first hydrochloric acid in mass percentage concentration, chloride is also contained in the primary washing water, hydroxide corresponding to cations of the chloride is insoluble in water, and the secondary washing water is primary washing water for removing chloride;
step two: introducing the chlorine into yellow phosphorus water, and absorbing the chlorine by the yellow phosphorus water to obtain a mixture of first phosphoric acid and third hydrochloric acid;
step three: reacting the mixture of the first phosphoric acid and the third hydrochloric acid with sulfuric acid cinder to obtain crude iron phosphate;
step four: dissolving the crude ferric phosphate with second hydrochloric acid, and filtering to obtain clear liquid;
step five: distilling the clear liquid to separate out an iron phosphate crystal product;
step six: washing the iron phosphate crystal product with secondary washing water subjected to electrolytic purification in the step I to obtain refined iron phosphate, and converting the secondary washing water into primary washing water;
step seven: and feeding the primary washing water generated in the step six into an electrolysis device for electrolysis.
According to the invention, after hydrochloric acid, phosphorus chloride, magnesium chloride and calcium chloride in the primary washing water are subjected to electrolytic reaction, chloride ions generate chlorine, the chlorine reacts with yellow phosphorus water to generate a mixture of first phosphoric acid and third hydrochloric acid, and the mixture of the first phosphoric acid and the third hydrochloric acid and sulfuric acid cinder generate crude iron phosphate, so that the sulfuric acid cinder is changed into valuable through recycling of the chloride ions, the discharge of the chloride ions is avoided to pollute the environment, cations are combined with hydroxyl to form precipitates to be discharged, the concentration of the cations is prevented from being increased continuously, the primary washing water subjected to electrolytic treatment can be recycled, and the zero emission of the washing water is realized.
Drawings
FIG. 1 is a flow chart of a method for wastewater treatment and recycling in iron phosphate production.
Fig. 2 is a schematic structural diagram of the evaporative condenser.
Fig. 3 is a schematic view of the structure of the boiling wall.
Fig. 4 is a schematic structural view of the condensation duct in a front view direction.
Fig. 5 is a schematic structural diagram of the condensing duct viewed from the right.
In the figure: the device comprises an evaporation pan 10, a water inlet pipeline 11, a first electromagnetic valve 111, a water outlet pipeline 12, a second electromagnetic valve 121, a condensation pipeline 13, a condensation part 131, a baffle plate 1311, a liquid level controller 14, a boiling wall 15, a heating furnace 20, a combustion chamber 21, a hydrogen pipeline 22, a water discharge pipeline 23 and a combustion-supporting gas pipeline 24.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
Referring to fig. 1, the embodiment of the invention provides a wastewater treatment recycling method in iron phosphate production, which comprises the following steps:
step S300: feeding the primary washing water into an electrolysis device for electrolysis to obtain chlorine, hydrogen, hydroxide precipitates and secondary washing water, discharging the hydrogen from a hydrogen discharge port, and discharging the hydroxide precipitates from an electrolysis bath; the method comprises the following steps of (1) preparing primary washing water, wherein the primary washing water is washing water containing 1-5% of first hydrochloric acid in mass percentage concentration, chloride is also contained in the primary washing water, hydroxide corresponding to cations of the chloride is insoluble in water, and the secondary washing water is primary washing water for removing chloride;
step S301: introducing chlorine gas into the yellow phosphorus water, and absorbing the chlorine gas by the yellow phosphorus water to obtain a mixture of first phosphoric acid and third hydrochloric acid, wherein the reaction I in the figure 1 refers to the reaction of the chlorine gas and the yellow phosphorus water;
step S302: reacting a mixture of the first phosphoric acid and the third hydrochloric acid with the sulfuric acid cinder to obtain crude iron phosphate, wherein the reaction in the figure 1 refers to the reaction of phosphoric acid and sulfuric acid cinder;
step S303: dissolving the crude ferric phosphate with second hydrochloric acid, and filtering to obtain clear liquid;
step S304: distilling the clear liquid, and separating out an iron phosphate crystal product;
step S305: washing the iron phosphate crystal product with secondary washing water subjected to electrolytic purification in the step S300 to obtain refined iron phosphate, and converting the secondary washing water into primary washing water;
step S306: the primary washing water generated in step S305 is fed into the electrolysis device again for electrolysis.
According to the invention, after hydrochloric acid, phosphorus chloride, magnesium chloride and calcium chloride in the primary washing water are subjected to electrolytic reaction, chloride ions generate chlorine, the chlorine reacts with yellow phosphorus water to generate a mixture of first phosphoric acid and third hydrochloric acid, and the mixture of the first phosphoric acid and the third hydrochloric acid and sulfuric acid cinder generate crude iron phosphate, so that the sulfuric acid cinder is changed into valuable through recycling of the chloride ions, the discharge of the chloride ions is avoided to pollute the environment, cations are combined with hydroxyl to form precipitates to be discharged, the concentration of the cations is prevented from being increased continuously, the primary washing water subjected to electrolytic treatment can be recycled, and the zero emission of the washing water is realized.
Further, in step S302, the mass percentage concentration of the first phosphoric acid in the mixture of the first phosphoric acid and the third hydrochloric acid is 20 to 80%.
Further, in step S303, the second hydrochloric acid has a mass percentage concentration of 20 to 30%.
Referring to fig. 1, further, the primary washing water in step S300 is subjected to a pretreatment step before electrolysis, wherein the pretreatment step is to pass the primary washing water through an evaporative condenser to concentrate the primary washing water with a mass percentage concentration of 1-5%, and the evaporative condenser is heated by using the hydrogen discharged in step S300.
In the embodiment, the hydrogen generated by the electrolysis reaction is used for evaporation and concentration of the primary washing water, so that the electrolysis efficiency of the primary washing water is improved, the electrolysis energy consumption is reduced, and meanwhile, the emission of the hydrogen is avoided to pollute the environment, and the energy waste is avoided.
Referring to fig. 2, further, the evaporative condenser includes an evaporation pan 10, a heating furnace 20, a hydrogen pipeline 22, a drainage pipeline 23, and a combustion-supporting gas pipeline 24 are installed on the heating furnace 20, a water inlet pipeline 11, a water outlet pipeline 12, a condensation pipeline 13, and a liquid level controller 14 are installed on the evaporation pan 10, the evaporation pan 10 passes through a circular hole on the top wall of the heating furnace 20 and is nested in the heating furnace 20, an outer circumferential wall of an upper portion of the evaporation pan 10 is fixed and hermetically connected with an inner circumferential wall of the circular hole on the top wall of the heating furnace 20, one end of the hydrogen pipeline 22 is communicated with the bottom of a combustion chamber 21 of the heating furnace 20, the other end of the hydrogen pipeline 22 is communicated with a hydrogen discharge port of an electrolysis device, a drainage pipeline 23 is communicated with the bottom of the combustion chamber 21 of the heating furnace 20 to discharge water generated after the combustion of hydrogen, the bottom of the combustion chamber 21 of the heating furnace 20 is communicated with the combustion-supporting gas pipeline 24 to introduce air into the combustion chamber 21 of the heating furnace 20, the upper part of the evaporative condenser is connected with a water inlet pipeline 11 to lead primary washing water to be pretreated into the evaporative condenser, a first electromagnetic valve 111 is arranged on the water inlet pipeline 11, the lower part of the evaporative condenser is connected with a water outlet pipeline 12 to lead the primary washing water after evaporation concentration into an electrolytic bath, a second electromagnetic valve 121 is arranged on the water outlet pipeline 12, after the water in the evaporative condenser is evaporated, water vapor forms condensed water at the top of the evaporative condenser, the condensed water is conveyed to a using point from a water outlet at the top of the evaporative condenser through a condensing pipeline 13 to wash an iron phosphate crystallization product, a liquid level controller 14 is arranged in the evaporative condenser, the liquid level controller 14 is electrically connected with a control module, the control module is electrically connected with the first electromagnetic valve 111 and the second electromagnetic valve 121, when the water level in the evaporative condenser is at a low water level, the liquid level controller 14 sends a low water level signal to the control module, the controller module controls the first electromagnetic valve 111 to be opened and the second electromagnetic valve 121 to be closed, when the water level in the evaporative condenser is at a high water level, the liquid level controller 14 sends a signal that the water level is high to the control module, and the control module controls the first electromagnetic valve 111 to be closed and the second electromagnetic valve 121 to be opened.
In this embodiment, the liquid level controller 14 controls the first electromagnetic valve 111 to close, and the second electromagnetic valve 121 to intermittently open or close, so as to control the liquid level of the primary washing water in the evaporative condenser, thereby indirectly controlling the mass percentage concentration of the hydrochloric acid in the pretreated primary washing water, so as to intermittently provide the primary washing water containing the hydrochloric acid required by the specified mass percentage concentration for the electrolysis apparatus.
Referring to fig. 2 and 3, further, the inside of the evaporative condenser has a boiling wall 15 contacting the primary washing water therein and heating the primary washing water, and fine protrusions are densely distributed on a side of the boiling wall 15 contacting the primary washing water, and free ends of the protrusions are disposed as tips.
In this embodiment, the evaporative condenser is in contact with water, and the part for heating the water is provided as the boiling wall 15, on the one hand, the evaporation area is increased by the densely arranged fine protrusions, and on the other hand, the free ends of the protrusions are provided as tips to provide growth nuclei for bubble production, thereby promoting the evaporation of the water.
Referring to fig. 2, 4 and 5, further, the cross section of the condensing duct 13 is square, a plurality of condensing parts 131 are uniformly inserted into the condensing duct 13 along the length direction thereof at intervals, the condensing parts 131 include two baffle plates 1311, the two baffle plates 1311 are arranged in a reverse inclined manner, and each baffle plate 1311 is trapezoidal and perpendicular to the inner side wall of the exhaust duct.
The baffling board 1311 adjusts the condition that flows of vapor in the condensation pipe 13, after the baffling board 1311 was touched to vapor, a small part of comdenstion water flowed down along baffling board 1311, a plurality of baffling boards 1311 have increased the heat transfer area of vapor simultaneously, the condensation of vapor has been accelerated, behind the condensate film on the baffling board 1311 to certain thickness, gather in condensation pipe 13 bottom along baffling board 1311 under the effect of gravity and air current, flow to the point of use again along condensation pipe 13 bottom, for washing iron phosphate crystallization product, the vapor condensation effect has effectively been accelerated, this condensation pipe 13 neither additionally increases equipment structure, again can make full use of the space in the pipeline of existing equipment, and reached the water vapor condensation effect with higher speed, the structure is simple and easy, and practical.
Further, the electrolysis process of the primary washing water in step S300 is to pass the pretreated primary washing water through a cation membrane electrolytic cell, obtain chlorine and hydrogen by using a copper mesh as a cathode and a titanium alloy as an anode, and the electrolysis is performed in a continuous multi-stage manner, that is, the primary washing water after the primary electrolysis is supplemented with new primary washing water for secondary electrolysis, and the primary washing water after the secondary electrolysis is supplemented with new primary washing water for tertiary electrolysis, and so on.
In the embodiment, the copper mesh is used as the cathode, so that the diffusion distance of chloride ions in the electrolyte can be effectively reduced, the electrolysis energy consumption is reduced, and the method is more suitable for preparing chlorine gas by electrolysis of low-concentration hydrochloric acid aqueous solution.
The steps in the method of the embodiment of the invention can be sequentially adjusted, combined and deleted according to actual needs.
The modules or units in the device of the embodiment of the invention can be combined, divided and deleted according to actual needs.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A method for treating and recycling wastewater in iron phosphate production is characterized by comprising the following steps:
the method comprises the following steps: feeding the primary washing water into an electrolysis device for electrolysis to obtain chlorine, hydrogen, hydroxide precipitates and secondary washing water, discharging the hydrogen from a hydrogen discharge port, and discharging the hydroxide precipitates from an electrolysis bath;
the method comprises the following steps of (1) preparing primary washing water, wherein the primary washing water is washing water containing 1-5% of first hydrochloric acid in mass percentage concentration, chloride is also contained in the primary washing water, hydroxide corresponding to cations of the chloride is insoluble in water, and the secondary washing water is primary washing water for removing chloride;
step two: introducing the chlorine into yellow phosphorus water, and absorbing the chlorine by the yellow phosphorus water to obtain a mixture of first phosphoric acid and third hydrochloric acid;
step three: reacting the mixture of the first phosphoric acid and the third hydrochloric acid with sulfuric acid cinder to obtain crude iron phosphate;
step four: dissolving the crude ferric phosphate with second hydrochloric acid, and filtering to obtain clear liquid;
step five: distilling the clear liquid to separate out an iron phosphate crystal product;
step six: washing the iron phosphate crystal product with secondary washing water subjected to electrolytic purification in the step I to obtain refined iron phosphate, and converting the secondary washing water into primary washing water;
step seven: and feeding the primary washing water generated in the step six into an electrolysis device for electrolysis.
2. The method for treating and recycling wastewater in the iron phosphate production according to claim 1, characterized by comprising the following steps: in the third step, the mass percentage concentration of the first phosphoric acid in the mixture of the first phosphoric acid and the third hydrochloric acid is 20-80%.
3. The method for treating and recycling wastewater in the iron phosphate production according to claim 1, characterized by comprising the following steps: in the fourth step, the mass percentage concentration of the second hydrochloric acid is 20-30%.
4. The method for treating and recycling wastewater in the iron phosphate production according to claim 1, characterized by comprising the following steps: and (3) pretreating the primary washing water in the step (I) before electrolysis, wherein the pretreatment step is to pass the primary washing water through an evaporative condenser to concentrate the primary washing water with the mass percentage concentration of 1-5%, and the evaporative condenser is heated by adopting the hydrogen discharged in the step (I).
5. The method for treating and recycling wastewater in the iron phosphate production according to claim 4, characterized by comprising the following steps: the evaporative condenser comprises an evaporating pot and a heating furnace, wherein a hydrogen pipeline, a drainage pipeline and a combustion-supporting gas pipeline are installed on the heating furnace, a water inlet pipeline, a water outlet pipeline, a condensation pipeline and a liquid level controller are installed on the evaporating pot, the evaporating pot penetrates through a circular hole in the top wall of the heating furnace and is embedded into the heating furnace, an outer ring wall on the upper portion of the evaporating pot is fixedly and hermetically connected with an inner ring wall of the circular hole in the top wall of the heating furnace, one end of the hydrogen pipeline is communicated with the bottom of a combustion chamber of the heating furnace, the other end of the hydrogen pipeline is communicated with a hydrogen discharge port of an electrolysis device, the bottom of the combustion chamber of the heating furnace is communicated with a drainage pipeline so as to discharge water generated after hydrogen combustion, the bottom of the combustion chamber of the heating furnace is communicated with the combustion-supporting, the device comprises an evaporative condenser, a water inlet pipeline, a water outlet pipeline, a water level controller, a control module, a first electromagnetic valve, a second electromagnetic valve, a water level controller, a first electromagnetic valve, a second electromagnetic valve, a water level controller, a first electromagnetic valve and a second electromagnetic valve, wherein the first washing water to be pretreated is introduced into the evaporative condenser, the water outlet pipeline is connected with the lower part of the evaporative condenser, the first washing water after evaporative concentration is introduced into an electrolytic bath, the second electromagnetic valve is arranged on the water outlet pipeline, after water in the evaporative condenser is evaporated, water vapor forms condensate water at the top of the evaporative condenser, the condensate water is conveyed to a use point through a condensation pipeline from a water outlet at the top of the evaporative condenser and is used for washing ferric phosphate crystallization products, the liquid level controller is arranged in the evaporative condenser and is electrically connected with the control module, the control module is electrically connected with the first electromagnetic valve and the second electromagnetic valve, and the control module sends a signal that the water level is low when the water level in the evaporative condenser is at a low water level, and the first electromagnetic valve is controlled by the control module to be opened, The second electromagnetic valve is closed, when the water level in the evaporative condenser is at a high water level, the liquid level controller sends a signal that the water level is high to the control module, the control module controls the first electromagnetic valve to be closed, and the second electromagnetic valve is opened.
6. The method for treating and recycling wastewater in the iron phosphate production according to claim 5, characterized in that: the inside of the evaporative condenser is provided with a boiling wall which is contacted with the primary washing water and is used for heating the primary washing water, one side of the boiling wall contacted with the primary washing water is densely distributed with fine bulges, and the free ends of the bulges are arranged to be tips.
7. The method for treating and recycling wastewater in the iron phosphate production according to claim 5, characterized in that: the cross-section of the condensation pipeline is square, a plurality of condensation parts are inserted into the condensation pipeline along the length direction of the condensation pipeline at uniform intervals, each condensation part comprises two baffle plates, the two baffle plates are arranged in a reverse inclined mode, and each baffle plate is trapezoidal and is perpendicular to the side wall of the inner side of the exhaust pipeline.
8. The method for treating and recycling wastewater in the iron phosphate production according to claim 1, characterized by comprising the following steps: and in the step one, the electrolysis process of the primary washing water comprises the steps of enabling the pretreated primary washing water to pass through a cationic membrane electrolytic cell, taking a copper net as a cathode and a titanium alloy as an anode to obtain chlorine and hydrogen, and adopting a continuous multi-stage mode, namely supplementing new primary washing water to the primary washing water subjected to primary electrolysis for secondary electrolysis, supplementing new primary washing water to the primary washing water subjected to secondary electrolysis for tertiary electrolysis, and so on.
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